技术领域technical field
本发明涉及分析化学技术领域，具体涉及一种液相色谱流动相预警装置。The invention relates to the technical field of analytical chemistry, in particular to a liquid chromatography mobile phase early warning device.
背景技术Background technique
液相色谱流动相通常是指各种低沸点溶剂和水溶液。与气相色谱比较，液相色谱流动相不仅可选择范围比较大，而且它是影响分离的一个非常重要的可调节因素。目前，常用的液相色谱仪的流动相分为极性类、非极性类、易挥发类、不易挥发类等，而盛放流动相的溶剂瓶大都是与空气相通的敞开式结构，敞开式结构对于常用的非挥发类的中性流动相来说没多大影响的，但对于易吸收空气中二氧化碳的而影响其PH 值的显碱性的流动相、有机相所占比例较大的易挥发的流动相、含易挥发的刺激性组分的流动相来说有较大的局限性。Liquid chromatography mobile phase usually refers to various low boiling point solvents and aqueous solutions. Compared with gas chromatography, liquid chromatography mobile phase not only has a wider selection range, but also is a very important adjustable factor affecting separation. At present, the mobile phases of commonly used liquid chromatographs are divided into polar, non-polar, volatile, non-volatile, etc., and the solvent bottles containing the mobile phase are mostly open structures that communicate with the air. The formula structure does not have much influence on the commonly used non-volatile neutral mobile phase, but it is easy to absorb carbon dioxide in the air and affect its pH value, which is alkaline mobile phase and organic phase. There are greater limitations for volatile mobile phases and mobile phases containing volatile and irritating components.
为解决上述问题，公开号为CN203635201U的中国专利公开了一种液相色谱用流动相盛放装置，该装置包括盛放流动相的广口瓶、具有可拆卸接头的进液管、具有阀门的弯管、具有进气口和出气口的塑料袋，所述广口瓶包括玻璃瓶本体和与玻璃瓶本体相匹配的瓶塞，瓶塞上具有分别与进液管和弯管相匹配的两个通孔，进液管伸入到广口瓶内的一端固定连接有玻璃砂芯过滤器，弯管的阀门处固定连接塑料袋的进气口，所述塑料袋的容积是广口瓶容积的一半。该技术方案具有较好的密封效果，可适用于易挥发类流动相，但是由于是采用塑料袋的瘪气来判断流动相是否用完，判断准确性较差，尤其是在塑料袋存在泄露或流动相产生气泡的情况下很难判断流动相是否用完，同时也不会产生预警，因此不能对流动相做出实时监测。In order to solve the above problems, the Chinese patent with the publication number CN203635201U discloses a mobile phase containing device for liquid chromatography. An elbow, a plastic bag with an air inlet and an air outlet. The jar includes a glass bottle body and a cork matching the glass bottle body. A through hole, one end of the liquid inlet pipe extending into the wide-mouth bottle is fixedly connected with a glass sand core filter, and the valve of the elbow is fixedly connected with the air inlet of the plastic bag, and the volume of the plastic bag is the volume of the wide-mouth bottle. half of. This technical solution has a good sealing effect and is applicable to volatile mobile phases. However, since the deflated plastic bag is used to judge whether the mobile phase is used up, the judgment accuracy is poor, especially when the plastic bag is leaked or When the mobile phase generates bubbles, it is difficult to judge whether the mobile phase is used up, and at the same time, no warning will be generated, so real-time monitoring of the mobile phase cannot be performed.
为了实现对液相色谱流动相的监视和提醒，公开号为CN 202734898 U的中国专利公开了一种用于液相色谱流动相的监视提醒装置，该装置是在流动瓶的底部设置称重模块，流动瓶上设有外部显示装置，借助外部显示装置醒目提示所盛流动相的剩余体积和更换时间；但是当温度或压力变化而导致流动相产生气泡时，显示装置不会做出提示或预警，因此造成系统发生故障，造成不必要的经济损失。In order to realize the monitoring and reminding of the mobile phase of liquid chromatography, the Chinese patent with the publication number CN 202734898 U discloses a monitoring and reminding device for the mobile phase of liquid chromatography. The device is to set a weighing module at the bottom of the flow bottle , the flow bottle is equipped with an external display device, with which the remaining volume of the mobile phase and the replacement time of the mobile phase can be clearly indicated; however, when the temperature or pressure changes and the mobile phase generates bubbles, the display device will not give a prompt or early warning , thus causing system failure and unnecessary economic losses.
发明内容Contents of the invention
本发明的目的在于克服现有技术所存在的不足，提供了一种液相色谱流动相预警装置。The purpose of the present invention is to overcome the deficiencies in the prior art and provide a liquid chromatography mobile phase early warning device.
本发明是通过如下技术方案予以实现的:The present invention is achieved through the following technical solutions:
一种液相色谱流动相预警装置，主要由液相色谱仪及智能控制系统组成，所述液相色谱仪包括泵以及通过管道依次连接的进样器、色谱柱、检测器和废液瓶，所述泵的输入端连接流动相盛放瓶，泵的输出端通过管道经进样器与色谱柱的输入端相连；所述智能控制系统包括温度传感器、压力传感器、PLC主机、PLC模块及触摸显示屏，所述PLC模块和PLC主机插接，所述温度传感器和压力传感器分别设置于流动相盛放瓶，通过PLC模块接受温度传感器和压力传感器采集的模拟量信号，转换成数字信号，由PLC主机送入触摸显示屏。A mobile phase early warning device for liquid chromatography, mainly composed of a liquid chromatograph and an intelligent control system, the liquid chromatograph includes a pump, a sampler, a chromatographic column, a detector and a waste liquid bottle connected in sequence through pipelines, The input end of the pump is connected to the mobile phase holding bottle, and the output end of the pump is connected to the input end of the chromatographic column through a sampler through a pipeline; the intelligent control system includes a temperature sensor, a pressure sensor, a PLC host, a PLC module and a touch screen. The display screen, the PLC module and the PLC host are plugged in, the temperature sensor and the pressure sensor are respectively arranged in the mobile phase holding bottle, and the analog signal collected by the temperature sensor and the pressure sensor is received by the PLC module, converted into a digital signal, and then converted into a digital signal by The PLC host sends it to the touch screen.
进一步地，所述流动相盛放瓶底部设置有与管道相连的过滤器。Further, a filter connected to a pipeline is provided at the bottom of the mobile phase holding bottle.
进一步地，所述智能控制系统还包括散热风扇、电源指示灯、异常指示灯及蜂鸣器。通过指示灯和蜂鸣器进行故障指示或报警。Further, the intelligent control system also includes a cooling fan, a power indicator light, an abnormal indicator light and a buzzer. Fault indication or alarm through indicator light and buzzer.
进一步地，所述过滤器采用玻璃砂芯过滤器。Further, the filter adopts a glass sand core filter.
进一步地，所述检测器采用电导检测仪。Further, the detector adopts a conductivity detector.
本发明的有益效果是：The beneficial effects of the present invention are:
与现有技术相比，本发明通过采用PLC智能控制系统实时监控流动相的工作温度及工作压力，避免流动相因温度升高或压力降低而导致气泡逸出，防止意外故障发生，提高了液相色谱仪的工作的安全性，避免造成不必要的经济损失。Compared with the prior art, the present invention monitors the working temperature and working pressure of the mobile phase in real time by adopting the PLC intelligent control system, avoids the escape of bubbles caused by the temperature rise or pressure drop of the mobile phase, prevents accidental failures, and improves the liquid quality. The safety of the work of the phase chromatograph and avoid unnecessary economic losses.
附图说明Description of drawings
图1为本发明结构示意图。Fig. 1 is a schematic diagram of the structure of the present invention.
其中图1中各部分为：The parts in Figure 1 are:
1-流动相盛放瓶；2-泵；3-进样器；4-色谱柱；5-检测器；6-计算机；7-废液瓶；8-温度传感器；9-压力传感器；10-PLC主机；11-PLC模块；12-触摸显示屏；13-过滤器。1-mobile phase holding bottle; 2-pump; 3-injector; 4-chromatographic column; 5-detector; 6-computer; 7-waste bottle; 8-temperature sensor; 9-pressure sensor; 10- PLC host; 11-PLC module; 12-touch display screen; 13-filter.
具体实施方式Detailed ways
下面结合附图进一步描述本发明的技术方案，但要求保护的范围并不局限于所述。The technical solution of the present invention is further described below in conjunction with the accompanying drawings, but the scope of protection is not limited to the description.
如图1所示，本发明所述的一种液相色谱流动相预警装置，主要由液相色谱仪及智能控制系统组成，所述液相色谱仪包括泵2以及通过管道依次连接的进样器3、色谱柱4、检测器5和废液瓶7，所述泵2 的输入端连接流动相盛放瓶1，泵2的输出端通过管道经进样器3与色谱柱4的输入端相连；所述智能控制系统包括温度传感器8、压力传感器9、PLC主机10、PLC模块11及触摸显示屏12，所述PLC模块11和PLC主机10插接，所述温度传感器8和压力传感器9分别设置于流动相盛放瓶1，通过PLC模块11接受温度传感器8和压力传感器9采集的模拟量信号，转换成数字信号，由PLC主机10送入触摸显示屏12，显示各种工作参数，从而实现对流动相的实时监控及预警。As shown in Figure 1, a liquid chromatography mobile phase early warning device according to the present invention is mainly composed of a liquid chromatography instrument and an intelligent control system. device 3, chromatographic column 4, detector 5 and waste liquid bottle 7, the input end of the pump 2 is connected to the mobile phase holding bottle 1, the output end of the pump 2 passes through the input end of the sampler 3 and the chromatographic column 4 through the pipeline Connected; the intelligent control system includes a temperature sensor 8, a pressure sensor 9, a PLC host 10, a PLC module 11 and a touch display screen 12, the PLC module 11 and the PLC host 10 are plugged, and the temperature sensor 8 and the pressure sensor 9 They are respectively arranged in the mobile phase holding bottle 1, and receive the analog signal collected by the temperature sensor 8 and the pressure sensor 9 through the PLC module 11, convert it into a digital signal, send it to the touch screen 12 by the PLC host 10, and display various working parameters, In this way, real-time monitoring and early warning of the mobile phase can be realized.
所述检测器5上还连接有计算机6。A computer 6 is also connected to the detector 5 .
采用上述技术方案，在应用时，液相色谱流动相携带被测试样品通过色谱柱4，泵2将流动相以稳定的流速（或压力）输送至分析体系；待测样品在色谱柱4 之前通过进样器3将样品导入，流动相将样品带入色谱柱4；在色谱柱4中，各组分因在固定相中的分配系数或吸附力大小的不同而被分离，并依次随流动相流至检测器5 ；检测器5将检测到的信号送至计算机6记录、处理或保存，从计算机6记录的数据即可计算得出试样中各种待测组分的浓度，并将废液排放至废液瓶7中。With the above-mentioned technical scheme, in application, the liquid chromatography mobile phase carries the sample to be tested through the chromatographic column 4, and the pump 2 delivers the mobile phase to the analysis system at a stable flow rate (or pressure); the sample to be tested passes through the chromatographic column 4 before The sample injector 3 introduces the sample, and the mobile phase brings the sample into the chromatographic column 4; in the chromatographic column 4, each component is separated due to the difference in distribution coefficient or adsorption force in the stationary phase, and is sequentially separated with the mobile phase. Flow to detector 5; Detector 5 sends the detected signal to computer 6 for recording, processing or preservation, and from the data recorded by computer 6, the concentration of various components to be measured in the sample can be calculated, and the waste The liquid is discharged into the waste liquid bottle 7.
在实际应用中，溶剂中能溶解气体的量随温度升高而降低，因而当溶剂从低温状态移至高温状态时，则过量溶解的气体会以气泡形式逸出；同时，当气体的分压增高时，气体在溶剂中的溶解量增大，在较高压力下达到饱和的溶液一旦压力下降必将产生气泡。本技术方案通过增加智能控制系统对流动相的温度和压力进行实时监控，以避免气泡的产生，其工作原理是：温度传感器8和压力传感器9将所测量到的温度和压力模拟量信号分别送至PLC模块11，经PLC模块11转换为相应的数字量信号，PLC主机10读取PLC模块11转换后的数字量信号并通过触摸显示屏12显示出来，以便于用户观察流动相的工作参数。同时用户通过对触摸显示屏12的操作来完成对流动相的工作状态的选择、工作参数的设定以及工作状态的监视；当流动相的温度或压力不满足设定要求时，由PLC控制系统停机，PLC主机10并将故障信号输出给PLC输出控制回路使指示报警回路工作，发出声光报警，同时通过触摸显示屏12显示故障现象和排除故障的方法。In practical applications, the amount of dissolved gas in the solvent decreases with the increase of temperature, so when the solvent moves from a low-temperature state to a high-temperature state, the excess dissolved gas will escape in the form of bubbles; at the same time, when the partial pressure of the gas When the pressure is increased, the amount of dissolved gas in the solvent increases, and the solution that reaches saturation at a higher pressure will inevitably produce bubbles once the pressure drops. This technical solution monitors the temperature and pressure of the mobile phase in real time by adding an intelligent control system to avoid the generation of air bubbles. Its working principle is: the temperature sensor 8 and the pressure sensor 9 send the measured temperature and pressure analog signals respectively To the PLC module 11, the PLC module 11 converts it into a corresponding digital signal, and the PLC host 10 reads the digital signal converted by the PLC module 11 and displays it on the touch screen 12, so that the user can observe the working parameters of the mobile phase. At the same time, the user completes the selection of the working state of the mobile phase, the setting of the working parameters and the monitoring of the working state through the operation of the touch screen 12; when the temperature or pressure of the mobile phase does not meet the setting requirements, the PLC control system Stop, the PLC host 10 outputs the fault signal to the PLC output control circuit to make the indication alarm circuit work, and sends out sound and light alarm, and displays the fault phenomenon and the method of troubleshooting through the touch screen 12 at the same time.
所述流动相盛放瓶1底部设置有与管道相连的过滤器13。The bottom of the mobile phase holding bottle 1 is provided with a filter 13 connected with a pipeline.
所述智能控制系统还包括散热风扇、电源指示灯、异常指示灯及蜂鸣器。通过指示灯和蜂鸣器进行故障指示或报警。The intelligent control system also includes a cooling fan, a power indicator light, an abnormal indicator light and a buzzer. Fault indication or alarm through indicator light and buzzer.
所述过滤器13采用玻璃砂芯过滤器。The filter 13 adopts a glass sand core filter.
所述检测器5采用电导检测仪。The detector 5 is a conductivity detector.
本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。The above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, rather than limiting the implementation of the present invention. For those of ordinary skill in the art, other changes or changes in different forms can be made on the basis of the above description. It is not necessary and impossible to exhaustively list all the implementation manners here. All modifications, equivalent replacements and improvements made within the spirit and principles of the present invention shall be included within the protection scope of the claims of the present invention.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410464890.1ACN104237427B (en) | 2014-09-12 | 2014-09-12 | A kind of liquid chromatogram mobile phase prior-warning device |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410464890.1ACN104237427B (en) | 2014-09-12 | 2014-09-12 | A kind of liquid chromatogram mobile phase prior-warning device |
| Publication Number | Publication Date |
|---|---|
| CN104237427Atrue CN104237427A (en) | 2014-12-24 |
| CN104237427B CN104237427B (en) | 2016-04-13 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410464890.1AExpired - Fee RelatedCN104237427B (en) | 2014-09-12 | 2014-09-12 | A kind of liquid chromatogram mobile phase prior-warning device |
| Country | Link |
|---|---|
| CN (1) | CN104237427B (en) |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108020606A (en)* | 2016-11-04 | 2018-05-11 | 罗斯蒙特分析公司 | The monitoring of analyzer component |
| CN111103367A (en)* | 2019-12-20 | 2020-05-05 | 刘仲 | Liquid chromatography mobile phase bottle with liquid drying recognition device |
| CN114651175A (en)* | 2019-11-20 | 2022-06-21 | 思拓凡瑞典有限公司 | Method for determining operating flow rate for a chromatography column in an HPLC system |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62167472A (en)* | 1985-11-29 | 1987-07-23 | Shimadzu Corp | Solvent supply device |
| JPS63165720A (en)* | 1986-12-26 | 1988-07-09 | Fujitsu Ltd | Liquid storage tank with liquid level alarm |
| JP2008215978A (en)* | 2007-03-02 | 2008-09-18 | Shimadzu Corp | Liquid feed pump and liquid chromatograph using the same |
| CN102171561A (en)* | 2008-10-06 | 2011-08-31 | 爱科来株式会社 | Analyzing device |
| CN102641711A (en)* | 2012-04-12 | 2012-08-22 | 山东创新药物研发有限公司 | Flowing phase containing device used for sealed liquid phase color spectrum |
| JP2013002815A (en)* | 2011-06-10 | 2013-01-07 | Ulvac Japan Ltd | Flow-through measuring device |
| CN202734898U (en)* | 2012-07-26 | 2013-02-13 | 尹磊 | Monitoring and reminding device used for flowing phase of liquid chromatogram |
| CN203397202U (en)* | 2013-08-30 | 2014-01-15 | 无锡衡联科技有限公司 | Real-time monitoring system used for enterprise production line |
| CN203705405U (en)* | 2014-02-26 | 2014-07-09 | 苏州环球色谱有限责任公司 | Liquid chromatographsystem |
| CN204065040U (en)* | 2014-09-12 | 2014-12-31 | 华南理工大学 | A kind of liquid chromatogram mobile phase prior-warning device |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62167472A (en)* | 1985-11-29 | 1987-07-23 | Shimadzu Corp | Solvent supply device |
| JPS63165720A (en)* | 1986-12-26 | 1988-07-09 | Fujitsu Ltd | Liquid storage tank with liquid level alarm |
| JP2008215978A (en)* | 2007-03-02 | 2008-09-18 | Shimadzu Corp | Liquid feed pump and liquid chromatograph using the same |
| CN102171561A (en)* | 2008-10-06 | 2011-08-31 | 爱科来株式会社 | Analyzing device |
| JP2013002815A (en)* | 2011-06-10 | 2013-01-07 | Ulvac Japan Ltd | Flow-through measuring device |
| CN102641711A (en)* | 2012-04-12 | 2012-08-22 | 山东创新药物研发有限公司 | Flowing phase containing device used for sealed liquid phase color spectrum |
| CN202734898U (en)* | 2012-07-26 | 2013-02-13 | 尹磊 | Monitoring and reminding device used for flowing phase of liquid chromatogram |
| CN203397202U (en)* | 2013-08-30 | 2014-01-15 | 无锡衡联科技有限公司 | Real-time monitoring system used for enterprise production line |
| CN203705405U (en)* | 2014-02-26 | 2014-07-09 | 苏州环球色谱有限责任公司 | Liquid chromatographsystem |
| CN204065040U (en)* | 2014-09-12 | 2014-12-31 | 华南理工大学 | A kind of liquid chromatogram mobile phase prior-warning device |
| Title |
|---|
| 张凯峰: "PLC在肉类行业腊肠生产工艺中的应用", 《包装与机械》, vol. 26, no. 6, 25 June 2005 (2005-06-25), pages 145 - 147* |
| 王浩 等: "基于PID调节的浴池恒温恒压供水系统", 《软件》, vol. 32, no. 3, 16 June 2011 (2011-06-16)* |
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108020606A (en)* | 2016-11-04 | 2018-05-11 | 罗斯蒙特分析公司 | The monitoring of analyzer component |
| EP3535578A4 (en)* | 2016-11-04 | 2020-06-17 | Rosemount Inc. | A method of monitoring the components of gas analyser |
| CN108020606B (en)* | 2016-11-04 | 2024-03-26 | 罗斯蒙特公司 | Monitoring of analyzer components |
| CN114651175A (en)* | 2019-11-20 | 2022-06-21 | 思拓凡瑞典有限公司 | Method for determining operating flow rate for a chromatography column in an HPLC system |
| CN111103367A (en)* | 2019-12-20 | 2020-05-05 | 刘仲 | Liquid chromatography mobile phase bottle with liquid drying recognition device |
| Publication number | Publication date |
|---|---|
| CN104237427B (en) | 2016-04-13 |
| Publication | Publication Date | Title |
|---|---|---|
| CN103383377B (en) | Testing and calibrating device for gas-dissolved-in-transformer-oil online monitoring system | |
| CN207457147U (en) | A kind of non-methane total hydrocarbons and benzene homologues on-line monitoring chromatograph | |
| CN104237427B (en) | A kind of liquid chromatogram mobile phase prior-warning device | |
| CN104792365A (en) | Sulfur hexafluoride gas quality field integrated detector and detection method | |
| CN203241404U (en) | Automatic multi-parameter chemical reagent filling device of water quality online analyzer | |
| CN204065040U (en) | A kind of liquid chromatogram mobile phase prior-warning device | |
| CN201637730U (en) | Split flow sampling device for liquid chromatograph | |
| CN108398366B (en) | A comprehensive detection and analysis system and method for compressed air quality in a power plant | |
| CN109283297B (en) | Independent calibration sampling system for hydrogen online analysis | |
| CN102628840B (en) | Method for detecting sampling efficiency device of volatile organic compounds sampled by charcoal tube needle | |
| CN102236002A (en) | A system and method for measuring N2O concentration in the atmosphere | |
| CN108195950A (en) | The dilution error detection device and its detection method of calibrating gas dilution device based on gas chromatograph | |
| CN103091416B (en) | Gas analyzing system and working method thereof | |
| CN203881388U (en) | Oil gas flowmeter | |
| CN102854267B (en) | Measuring method of trace oxy-compound in liquid-phase propylene | |
| CN203337539U (en) | Device for automatically analyzing ozone concentration by use of ultraviolet spectrometry absorption technology | |
| CN203037629U (en) | Liquid chromatograph | |
| CN206862968U (en) | Alternating temperature concentrates electronics gas chromatography system | |
| CN204389331U (en) | The simple and easy adsorption/desorption device of use for laboratory | |
| CN213903313U (en) | Device for detecting content of mineral oil in sulfur hexafluoride gas | |
| CN203216909U (en) | Gas analysis system | |
| CN208091862U (en) | A kind of power plant's compressed air gaseous mass comprehensive detection and analysis system | |
| CN205374113U (en) | Volatile organic compounds's sampling system | |
| CN204462090U (en) | Oil component automatic separation equipment | |
| CN204330695U (en) | Program control transformer oil mixes gas, oil filtering system |
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee | Granted publication date:20160413 Termination date:20210912 |